CN103422170B - A kind of disc magnesium fluoride MgF 2crystal coating material and production method thereof - Google Patents
A kind of disc magnesium fluoride MgF 2crystal coating material and production method thereof Download PDFInfo
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- CN103422170B CN103422170B CN201310323878.4A CN201310323878A CN103422170B CN 103422170 B CN103422170 B CN 103422170B CN 201310323878 A CN201310323878 A CN 201310323878A CN 103422170 B CN103422170 B CN 103422170B
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Abstract
The present invention relates to optical filming material field, particularly relate to a kind of disc magnesium fluoride MgF
2crystal coating material and production method thereof, is characterized in that, this material is a kind of water white polycrystalline optical crystal, and at wavelength 500mm place, its specific refractory power Ne=1.38, density of material is about 3.17 grams/cm
3; The shape of this material adapts to the diameter of all size electron beam gun crucible or crucible lining and the disc of depth design processing or circular cone cylindricality, and its diameter dimension scope is 20mm ~ 56mm, and gauge scope is: 5mm ~ 30mm.Compared with prior art, the invention has the beneficial effects as follows: meet electron beam gun plating MgF completely
2the dimensional requirement of film crucible, dress feeding is very convenient, have and really do not splash, do not collapse point, without discharge quantity and the excellent evaporation characteristic such as generating surface is smooth, effectively improve plated optical element surface smooth finish, be particularly useful for the ultra-smooth optical element surface plated film of high quality plated film requirement.<!--1-->
Description
Technical field
The present invention relates to optical filming material field, particularly relate to a kind of disc magnesium fluoride MgF
2crystal coating material and production method thereof.
Background technology
MgF
2splashing in vacuum plating and collapse the smooth finish that a phenomenon can have a strong impact on plated optical surface, this is the global problem being difficult to thoroughly solve always.The eighties latter stage, Britain and Germany, successively by advanced synthesis method of purification, prepare white powder MgF
2, its chemical purity is 99.99%, substantially solves MgF
2the excessive spatter of plated film, collapse a problem, but this Powdered MgF
2be only applicable to the resistance-type evaporation in vacuum plating, electron beam gun plated film can not be used for.
1997, Chinese Changchun ray machine pass through vacuum sintering method, develop " particle MgF
2crystal coating material ", its quality is the leading level in the world, but because of its processing condition instability, still thoroughly could not solve and splash and collapse a problem, the large particle of diameter 6-70 μm also happens occasionally.And granular MgF
2crystal coating material fills in electron beam gun plated film crucible to be got very inconvenient, also can cause artifact pollution, and this is also cause in plated film the another kind of factor of splashing and collapsing a little.
Along with the development of electron beam gun plated film, through colding pressing, after hot pressing and pressure, sintering method forms that the various Coating Materials of disc is corresponding to appear on the market, as ZrO
2, MgO, TiO
2, Al
2o
3+ ZrO
2, Al
2o
3the huge number such as+MgO, its object is drawn materials just as electron beam gun crucible size exactly, and dress is got conveniently, not easily pollute, and in evaporation, discharge quantity is few, therefore obtains widespread use.
Because electron beam gun plated film is to MgF in production
2the strict quality requirement that Coating Materials has " do not splash, do not collapse a little ", usually by high-purity MgF
2material is through Leng Ya ﹑ hot compacting, then the disc MgF prepared by method through sintering
2material can not use at all.Within 2007, Japan once developed a kind of opaque " white disc MgF
2coating Materials ", after colding pressing, sintering processes forms exactly, enter at that time Chinese market once fast-selling for the moment, can shortly same because of inner quality not good enough, splash and collapse a little seriously and discharge quantity is large etc. that problem is withdrawn from the market very soon.
" disc MgF
2crystal coating material " be the Coating Materials that vast plated film worker suddenly expects use always.Angle is taken into account, " disc MgF from making method and cost two aspect
2crystal " MgF of various diameter must be come from
2rod crystal, then shapes through optical-mechanical.
" the particle MgF of widespread use at present
2crystal coating material " vacuum sintering making method, due to be large crucible adopt in type of heating, crucible is heated seriously unbalanced, cannot make qualified MgF
2rod crystal.
The method of crystal manufactured by general descending manner single crystal growing furnace, can sinter out MgF with excellent hole crucible
2rod crystal and is monocrystalline, but limits Shou Heng warm area and pull down mechanism due to body of heater, and its crucible is all little, is generally Ф 300mm at diameter, high about 350mm, the MgF sintered out
2rod amount of crystals and limited length, its weight is no more than 20 kilograms at most, and length consuming time, and power consumption is large, involves great expense, if shape as disc MgF
2crystal per kilogram price will more than 5000 yuan, and therefore it can only be used for optical element and cannot be used for vacuum plating at all.That these reasons cause " disc MgF
2crystal coating material " can not appear on the market and apply so far.
Summary of the invention
The object of this invention is to provide a kind of disc magnesium fluoride MgF
2crystal coating material and production method thereof, for electron beam gun plated film, have not the splashing of Coating Materials, do not collapse point, without discharge quantity and the generating surface excellent evaporation characteristic such as smooth, and coating process dress feeding is convenient, can avoid because dress feeding causes artifact pollution.
For achieving the above object, the technical solution used in the present invention is:
A kind of disc magnesium fluoride MgF
2crystal coating material and production method thereof, this material is a kind of water white polycrystalline optical crystal coating material, and at wavelength 500mm place, its specific refractory power Ne=1.38, density of material is about 3.17 grams/cm
3; The shape of this material adapts to disc that the diameter of plurality of specifications electron beam gun crucible or crucible lining and depth design process or circular cone cylindricality, and its diameter dimension scope is 20mm ~ 56mm, and gauge scope is: 5mm ~ 30mm;
The making method of this material comprises vacuum sintering magnesium fluoride rhabdolith and optical-mechanical formed machining two operations, wherein: 1) process of vacuum sintering magnesium fluoride rhabdolith is:
1. heat up: magnesium fluoride powder is added in vaccum sintering device and vacuumizes, be provided with how excellent hole plumbago crucible in this vaccum sintering device and be equipped with graphite heater inside and outside crucible, after in device, vacuum tightness reaches 2Pa, heat inside and outside crucible is implemented simultaneously, and with 100 DEG C ~ 120 DEG C/h ramp, 10 ~ 12h, make temperature in device reach 1050 DEG C ~ 1200 DEG C;
2. constant temperature: keep vacuum tightness at 0.2 ~ 0.06Pa in device, temperature 1250 DEG C ~ 1260 DEG C, keeps constant temperature 14 ~ 16h;
3. lower the temperature: in device, keep vacuum tightness at 0.06 ~ 0.004Pa, with the speed of 20 DEG C ~ 25 DEG C/h cooling 30 ~ 32h; When device temperature reaches 640 DEG C ~ 600 DEG C, stop heating, apparatus body naturally cools to room temperature;
2) optical-mechanical formed machining process is:
From vaccum sintering device, take out the magnesium fluoride rhabdolith sintered, the diameter served as a contrast according to required electron beam gun crucible or crucible and the degree of depth get the MgF of corresponding size
2rhabdolith, by the wafer type MgF of design
2the specification of crystal coating material carries out optical-mechanical forming process:
1. first through inside diameter slicer the MgF of respective diameters size
2rhabdolith is cut into the wafer type MgF of certain thickness and certain thickness tolerance by size
2;
2. by the MgF of this thickness
2disk reaches the disk of intended diameter size through optics edge polisher tarry matter, and its smooth finish should reach ▽ more than 6;
3. last by shaping MgF
2disk cleans through Ultrasonic Cleaners, and baking box is dried and vacuum packaging, is final disc magnesium fluoride crystal Coating Materials product.
Described Coating Materials product is applicable to all electron beam gun plating MgF
2film, is particularly useful for the ultra-smooth optical element surface plating MgF that surface smoothness is better than 5/20
2film, plated film particle diameter can be less than 5 μm.
Compared with prior art, the invention has the beneficial effects as follows:
1) present invention wafer type MgF
2the specification of crystalline material processes according to all kinds of electron beam gun crucible or crucible lining size design, meets electron beam gun plating MgF completely
2the dimensional requirement of film crucible, dress feeding very facilitates and can avoid artifact pollution.
2) through MgF that secondary-cleaned vacuum sintering goes out
2rod crystal, its inner quality is excellent, comparatively " particle MgF
2crystal coating material " purity is higher, and chemical purity is greater than 99.99%, MgF
2mgO and Mg(OH in crystal)
2be eliminated more at the bottom of Toru, can exempt 6-70 μm in plated film large diameterly collapses a little, and effectively minimizing diameter less than 5 μm collapses point (disregarding less than 5 μm during current quality inspection to collapse a little), have and really do not splash, do not collapse point, without discharge quantity and the excellent evaporation characteristic such as generating surface is smooth, effectively can improve plated optical element surface smooth finish.The present invention is especially suitable for the ultra-smooth optical element surface plating MgF of high quality plated film requirement
2film.
3) product cost of the present invention is far below traditional descending manner single crystal growing furnace MgF
2rod crystal product (being only 1/5th of this cost), makes " disc MgF
2crystal coating material " can accept by the application of vast electron beam gun plated film field, and become high-grade magnesium fluoride crystal plated film novel material and appear on the market.
Accompanying drawing explanation
Fig. 1 is a kind of electron beam gun crucible sectional view in current electron beam gun coating equipment;
Fig. 2 is the disc MgF of the present invention for this electron beam gun crucible
2crystal sectional view;
Fig. 3 is the circular cone cylindricality MgF of the present invention for this electron beam gun crucible
2crystal sectional view.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described:
A kind of disc magnesium fluoride crystal of the present invention Coating Materials is a kind of water white polycrystalline optical crystal, and at wavelength 500mm place, its specific refractory power Ne=1.38, density of material is about 3.17 grams/cm
3; The shape of this material adapts to the diameter of all size electron beam gun crucible or crucible lining and the disc of depth design processing or circular cone cylindricality, and its diameter dimension scope is 20mm ~ 56mm, and its gauge scope is: 5mm ~ 30mm;
The making method of this material comprises vacuum sintering magnesium fluoride rhabdolith and optical-mechanical formed machining two operations, wherein: 1) process of vacuum sintering magnesium fluoride rhabdolith is:
1. heat up: magnesium fluoride powder is added in vaccum sintering device and vacuumizes, be provided with how excellent hole plumbago crucible in this vaccum sintering device and be equipped with graphite heater inside and outside crucible, after in device, vacuum tightness reaches 2Pa, heat inside and outside crucible is implemented simultaneously, and with 100 DEG C ~ 120 DEG C/h ramp, 10 ~ 12h, make temperature in device reach 1050 DEG C ~ 1200 DEG C;
2. constant temperature: keep vacuum tightness at 0.2 ~ 0.06Pa in device, temperature 1250 DEG C ~ 1260 DEG C, keeps constant temperature 14 ~ 16h;
3. lower the temperature: keep vacuum tightness at 0.06 ~ 0.004Pa in device, with the speed of 20 DEG C ~ 25 DEG C/h cooling 30 ~ 32h, when unit temp drops to 640 DEG C ~ 600 DEG C, stop heating, device naturally cools to room temperature;
2) optical-mechanical formed machining process is:
From vaccum sintering device, take out the magnesium fluoride rhabdolith sintered, the diameter served as a contrast according to required electron beam gun crucible or crucible and the degree of depth get the MgF of corresponding size
2rhabdolith, by the wafer type MgF of design
2the specification of crystal coating material carries out optical-mechanical forming process:
1. first through inside diameter slicer the MgF of respective diameters size
2rhabdolith is cut into the disc MgF of certain thickness and certain thickness tolerance by size
2;
2. by the MgF of this thickness
2disk reaches the disk of intended diameter size through optics edge polisher tarry matter, and this disc magnesium fluoride crystal surface smoothness should reach ▽ 6;
3. the last MgF that will be shaped
2disk cleans through Ultrasonic Cleaners, and baking box is dried and vacuum packaging, is final disc magnesium fluoride crystal Coating Materials product.
Seeing Fig. 1, is a kind of electron beam gun crucible sectional view in current electron beam gun coating equipment.
Seeing Fig. 2, is the disc MgF of the present invention for Fig. 1 electron beam gun crucible
2crystal sectional view.
This its diameter dimension of disc magnesium fluoride crystal Coating Materials has Ф 20mm ~ 56mm different size, and its gauge can not be 1/2,1/3,1/4 of the crucible degree of depth not etc., needs specification for 5mm ~ 30mm is various.
Seeing Fig. 3, is the circular cone cylindricality MgF of the present invention for Fig. 1 electron beam gun crucible
2crystal sectional view.
Due to " the disc MgF of various diameter and thickness
2crystal coating material " with electron beam gun crucible used or crucible lining match specifications; make coating process fill feeding and visual evaporating state all very convenient; product price is moderate; have again do not splash, Beng Dian ﹑ is not without discharge quantity and the excellent evaporation characteristic such as generating surface is smooth; therefore effectively can improve coated product quality and finished product rate, and appear on the market and widespread use as the magnesium fluoride crystal plated film novel material of top grade.
MgF of the present invention
2crystal coating novel material material product is specially adapted to the optical element surface plating MgF that surface smoothness is better than 5/20
2film, ensures that plated film particle diameter is less than 5 μm.
Claims (3)
1. a disc magnesium fluoride MgF
2the production method of crystal coating material, is characterized in that, described disc magnesium fluoride MgF
2crystal coating material is a kind of water white polycrystalline optical crystal coating material, and at wavelength 500nm place, its specific refractory power Ne=1.38, density of material is 3.17 grams/cm
3; The shape of this material adapts to the disc that the diameter of plurality of specifications electron beam gun crucible or crucible lining and depth design process, and its diameter dimension scope is 20mm ~ 56mm, and gauge scope is: 5mm ~ 30mm;
The making method of described Coating Materials comprises vacuum sintering magnesium fluoride rhabdolith and optical-mechanical formed machining two operations, wherein: 1) process of vacuum sintering magnesium fluoride rhabdolith is:
1. heat up: magnesium fluoride powder is added in vaccum sintering device and vacuumizes, be provided with how excellent hole plumbago crucible in this vaccum sintering device and be equipped with graphite heater inside and outside crucible, after in device, vacuum tightness reaches 2Pa, heat inside and outside crucible is implemented simultaneously, and with 100 DEG C ~ 120 DEG C/h ramp, 10 ~ 12h, make temperature in device reach 1050 DEG C ~ 1200 DEG C;
2. constant temperature: keep vacuum tightness at 0.2 ~ 0.06Pa in device, temperature 1250 DEG C ~ 1260 DEG C, keeps constant temperature 14 ~ 16h;
3. lower the temperature: in device, keep vacuum tightness at 0.06 ~ 0.004Pa, with the speed of 20 DEG C ~ 25 DEG C/h cooling 30 ~ 32h; When device temperature reaches 640 DEG C ~ 600 DEG C, stop heating, apparatus body naturally cools to room temperature;
2) optical-mechanical formed machining process is:
From vaccum sintering device, take out the magnesium fluoride rhabdolith sintered, the diameter served as a contrast according to required electron beam gun crucible or crucible and the degree of depth get the MgF of corresponding size
2rhabdolith, by the wafer type MgF of design
2the specification of crystal coating material carries out optical-mechanical forming process:
1. first through inside diameter slicer the MgF of respective diameters size
2rhabdolith is cut into the wafer type MgF of certain thickness and certain thickness tolerance by size
2;
2. by the MgF of this thickness
2disk reaches the disk of intended diameter size through optics edge polisher tarry matter, and its smooth finish should reach ▽ more than 6;
3. last by shaping MgF
2disk cleans through Ultrasonic Cleaners, and baking box is dried and vacuum packaging, is final disc magnesium fluoride crystal Coating Materials product.
2. a kind of disc magnesium fluoride MgF according to claim 1
2the production method of crystal coating material, is characterized in that, the Coating Materials product that described production method is produced is applicable to all electron beam gun plating MgF
2film.
3. a kind of disc magnesium fluoride MgF according to claim 2
2the production method of crystal coating material, is characterized in that, the Coating Materials product that described production method is produced is applicable to the ultra-smooth optical element surface plating MgF that surface smoothness is better than 5/20
2film, plated film particle diameter is less than 5 μm.
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| CN201310323878.4A CN103422170B (en) | 2013-07-29 | 2013-07-29 | A kind of disc magnesium fluoride MgF 2crystal coating material and production method thereof |
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|---|---|---|---|
| CN201310323878.4A CN103422170B (en) | 2013-07-29 | 2013-07-29 | A kind of disc magnesium fluoride MgF 2crystal coating material and production method thereof |
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| CN103422170B true CN103422170B (en) | 2016-03-30 |
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| CN104790025A (en) * | 2015-04-14 | 2015-07-22 | 营口市荣兴达科技实业有限公司 | Preparation device and preparation technology for magnesium fluoride single crystal coating material |
Citations (6)
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|---|---|---|---|---|
| JP2000211999A (en) * | 1999-01-22 | 2000-08-02 | Canon Inc | Production of fluoride |
| JP2006036619A (en) * | 2004-07-27 | 2006-02-09 | Soratesu Lab:Kk | Method and apparatus for manufacturing material |
| CN201289302Y (en) * | 2008-11-03 | 2009-08-12 | 长春晶科光电有限公司 | Device for heating stove stock in crucible |
| CN101850995A (en) * | 2010-06-18 | 2010-10-06 | 承德创为光电材料有限公司 | Process for preparing 5-20mm high-purity polycrystalline magnesium fluoride by liquid crystallization method |
| CN102674410A (en) * | 2011-03-09 | 2012-09-19 | 多氟多化工股份有限公司 | Production method for high-purity magnesium fluoride crystal |
| CN103147119A (en) * | 2013-03-21 | 2013-06-12 | 北京雷生强式科技有限责任公司 | Preparation method and growth equipment of magnesium fluoride crystal |
-
2013
- 2013-07-29 CN CN201310323878.4A patent/CN103422170B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000211999A (en) * | 1999-01-22 | 2000-08-02 | Canon Inc | Production of fluoride |
| JP2006036619A (en) * | 2004-07-27 | 2006-02-09 | Soratesu Lab:Kk | Method and apparatus for manufacturing material |
| CN201289302Y (en) * | 2008-11-03 | 2009-08-12 | 长春晶科光电有限公司 | Device for heating stove stock in crucible |
| CN101850995A (en) * | 2010-06-18 | 2010-10-06 | 承德创为光电材料有限公司 | Process for preparing 5-20mm high-purity polycrystalline magnesium fluoride by liquid crystallization method |
| CN102674410A (en) * | 2011-03-09 | 2012-09-19 | 多氟多化工股份有限公司 | Production method for high-purity magnesium fluoride crystal |
| CN103147119A (en) * | 2013-03-21 | 2013-06-12 | 北京雷生强式科技有限责任公司 | Preparation method and growth equipment of magnesium fluoride crystal |
Non-Patent Citations (2)
| Title |
|---|
| 多孔体坩埚生长氟化钙晶体;沈永宏;《光学精密工程》;20071031;第14卷(第10期);1474-1477 * |
| 氟化镁晶体的应用研究进展;王丽平等;《材料导报Ａ：综述篇》;20130531;第27卷(第5期);38-41 * |
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